Process of treating minerals



May 25., 1926.

*l 1,586,365 E. B. HIGGINS K RocE-ss 0F' TREATING MINERALS i FiledJune 20, 1925 3 sheets-sheet 1 May 425 1926;

- 1,586,365 E. B. HIGGINS PROCESS OF TREATING MINERALSv Filed June 20, 1925 s sheets-sneer 5 with suitable porosity.

Patented May 25, 1926.

UNITED STATES PATENT oFEicE.

ERIC BERKELEY` HIGGINS 0F LONDON, ENGLAND, ASSIGNOE T0 'UNITED WATER SOFTENERS LIMITED, OF LONDON, ENGLAND, BRITISH COMPANY.

PRooEss 0E TREATINC; MINERALS.

App'iication med :une 2o,

This invention relates to the treatment of granularl or powderedmaterials consisting of grains or particles of varying sizes with a view to grading the material or separating the constituent parts of different sizes. The

invention has particular reference to the treatment of base exchange zeolite-like inatei-ials and particularly to a process for the separation of the useful portion of such materials from the mineral deposit from which they, are obtained. The product in the natural condition, for example-in the case of glauconite, exchange substance itself varying quantities of. bodies which are inactive as regards base exchange and' such bodies must be separated from the base exchange material proper before the latter can be used for practical purposes. y

' Furthermore, the base exchange material itself occurs in varying degrees of fineness and it is desirable that the finer grades of this material shall be separated from those in a coarser state of subdivision in order that filter beds may subsequently b e obtained of the active base exchange material The coarser particles are in practice more useful When'mployed inthe usual type of base exchange apparatus.

The inactive impurities which so far have caused the greatest difficulty in separation from the glauconite are the clay-like bodies` which are retained by the base Aexchange material with the utmost tenacity. The raw g glauconite as obtained from theinineral deposit may be washed in a rapid stream of water, for example, 10 cwt. of the raw material may be washed in 1000 gallons of water per hour in a shelved rotating drum and after three hours an effluent is obtained which is still strongly contaminated with the claylike materials to an extent which 'is sufficient toV make it impossible to use the material iii commercial water `treatment even after the lauconite has been subjected to a stabilizing treatment, for example, by baking without subsequent separation of the finely divided impuriies by Washing and so forth.

It is the main object of the present invention in its application to the purification of base exchange materials, to separatey the contains in addition to the base:

1925,. Serial No; 38,525, and in Great Britain September 10, 1924.

n o l clay-impurities from the base exchange inaterial extremely rapidly by means of a inechanicalseparating treatment and preferably by means of a chemical treatment first and the invention alsoaims at making it possible to use a small volume of washing Water and in cases in which it is found necessary, to grade the base exchange material proper in accordance with its own size of grains with great economy in labour andy mechanical power.

According to the present invention, raw material to be graded is allowed to fall 'through one or more columns of liquid which itself is maintained in motion at a steady velocity, arranged so that the said velocity is greater than the natural rate of fall of the lighter constituents which itis desired to separate from the coarser, so

that the finer or lighter constituents are rethe l moved in the direction of fiow of the liquid from the coarser portions which fall against the direction of flow of the liquid. In the case of the raw glauconitetlie material is subjected, preferably after rough screening, tothe action of a solution which is faintly alkaline, such as sodium carbonate or causticsoda, or it may be even of common salt of such .a strength that the 'solution exerts a peptising action and defiocculates the claylke impurities, subsequent to which the material is subjected to the'lselective mechanical action of one or more columns of4 liquid which may be weak alkaline solution, this treatment being carried out as indicated above, Even in the case of such base exchange materials as glauconite, however,

a veryconsiderable separation of the liner undesirable constituents .is effected even Without the peptising chemical action above referred to-. When the material is subjected to the action of two or more columns in succession, the rates or flow of the solution in the two columns is made diferent,.the speed inthe second column being greater so that' in the seco-nd column it is -only really the trom sacks.

some examples of plant. for carrying out the invention will be ,lescribed more fully with reference to the accompanying dra\\'ings,- wherein Figure l isa side elevation ot' a preferred -formel" plant l'or the treatment ot raw glauconite, in accordance with the invention;

Figure 2 is a side elevation showing purely diagranunatically a plant in which the process is slightly' moditicd .Figure 3 is a similar diagram showing a process in which there is a passage through two separating columns in series;

Figure 4 is a similar diagram ot a l'urthcr moditieation in which there are three separatingl columns, and linally Figure 5 is a diagram showing a numher ot` separating columns incor]' orated in a single unit ofthe apparatus,

llefei'ring lirstfot all to Figure 1. l is a pit in which the raw n'lauconite is placed It is a pit at the toot of a bucket elevatorl Q. the latter carrying the `glauconite to the top and depositing the material upon a tray The glauconite from this tray slides on to a shaker screen 4 oscillated by means ot a crank The coarse refuse does not pass through the screen 4. but lalls oil at the forward edge through a chute .G tor the waste material. The liner portions containing the glauconite capable of use in water softening pass through the screen 4 on to a mixing chute 7. It is washed from that chute by means of the peptising solution passingl up through a pipe S into a tubular mixer 9 provided with rings of teeth l() by means of which it is maintained in continuous steady rotation. It is in this form ot' apparatus in this mixer tube wherein peptising ot the clay-like constituents takes fplaee.

lt has already been said that the may take place by means of faintly alkaline solution, or by mans ot' a solution ot common salt. The strength of the alkaline solu tion necessary varies somewhat according to the source ot the material and should in practice be verilied -by direct tests in the laboratory upon the material to be treated. It is found, however, to he ot the magnitude ot' live to titty times millinormal strength. For example. with one sample of American glauconite three-quarters ot a pound ot austic soda per ton of water 'as t'ound to bc the most suitable strength of alkali in the solution. In. any particular instance. however, the concentration of the solution for peptisation is usually confined to a fairly7 narrow range. It the concentration ol alkali is increased. the clay passes progressively from the condition ol tiocculation up to a maximum condition ot' peptisation and then iack again to llocculation. In practice it is -only necessary that the whole mass of the material shall be thoroughly.wetteth but excess over the minimum amount of alkaline solution in the tube 9 has no deleterious eltect upon the material as regards the peptisation phenomenon in itselt'. The amount otl alkaline solution ot' the strength mentioned above which is allowed to pass through the mixer tube t) 20() gallons per ton of glauconite passing trom the chute T into the tube il.

The wet material passes from the mixer tube t) into the separating column. This consists of a riser pipe ll sui-mounted by a pair ot cones, the central cone l2 being adlinstable vertically relativelyto the outer cone l!) for a purpose which will be referred to below. The outer eoneilz is flanged at its lower end and bolted to the top ot' the riser pipe ll and is also surrounded by a tank il. he wet glauconite is delivered into the upper end of the central cone l2 and t'alls down into the riser pipe 1l. ln the latter there is a steady upward tlow of water produced by means ol a centrifugal pump lo. lt has been l'ound that it' the soaked mass be allowed to .tall vertically hy virtue ot' its own density into a column otwater moving upwards at a velocity ol' 1.75 centi-- meters per second. all the constituents includingI clay and the tine `grades` ot base e1'- change material which on account ot their tinencss are not suitable ior use in the tilter beds as. most generally employed with basey exchange materials. will be carried upwards with the stream ot water. This results because their natural rate oll fall i'n water is less than 1.75 centimeters per second. `On he other hand, the coarser particles will continue to fall in the opposite direction to the tlow ot the liquid. ln this manner a separation is clieeted, the completeness ol` which depends upon the maintenance of comtaut conditions. particularly as to the l'low of the liquid and the vsupply oll the soaked glauconite. although eddy current movements and similar irregularities in the upward flow ol the column of water lshould be'avoided and other conditions should hc observed, such as the avoidance ol' two large a proportion of solid matter in the ascending liquid column together with a suiicient diameter ot the ascending column to eliminate' considerable skin friction ell'eet's having regard to the velocity ot' flow ot the liquid and to the time over which the material is submitted to the selective action ol' the water column; the latter. of course, depends upon the length ot' the column.

At the foot of the riser pipe ll there is'an expanded space formed by a conical vessel 16 int-o which the inlet pipe 1T for the water passes at the toot. '.lhe purpose of this is to enable the water to be admitted without setting up considerable eddy currents. The coarser material'lalls into this vessel and is discharged in the form ol a continuous Sli . tion of the water entering through the pipe' 17. The pulp from the pipe 18 falls into rectangular bins 19 and is there partly dried and is ready for carting away.

The lighter constituent parts rise up with the column of liquid in the pipe 11 and over- How at the-vedgeof the outer cone 13 into the tank 14. Thus these materials and the liquid pass through the annular space between the cones`12 and 13 and the crosssection of this annular space may be accurately adjusted by raising or lowering the central cone 12 relatively to the cone 13. The liquid with the lighter constituents passes down through one or other of the out-V i let' pipes 20 and 20b intoone or other of the cylindrical recepacles 21n or 21h. Two such receptacles are used so that the process can be continuous, one receptacle being'in use while the other is being emptied. For this purposethe pipes 20a and 2Ob each have a valve (not shown in' the drawings) enabling either one of the receptacles to be cut out of action at any time. Again, the provision of two receptacles 21n and 21b enables a` single apparatus to be used for washing two different materials. For example', glauconite can be washed and the fine material received in one of the receptacles when the starting material is raw glauconite and subsequently glauconite Whichwhas previously been stabilized by baking can be washed and the separated fine material received inthe other receptacle.

The greater part of the fine material is left in either thereceptacle 21u or the re* ceptacle 21", but the Water passing in with 1t together with a certain quantity of very fine mud passes out through a pipe 22 or 22b into a tank 23 which is furnished with a weir 24; over which the liquid escapes into a further tank 25. Thespurp'se of this Weir is to enable the velocity of How of the water through the apparatus to be checked. Obviously it is no use inserting aineter in the pipe 17 as the Water passing through that pipe does not all rise through-the riser pipe 11, part of it passes out with the sand through the pipe 18. y

If the supply of water for the peptising solution through the pipe 8 be hard it may be rendered free from line products which are harmful to the process and alkali may be economized by previous treatment. of the Water supply by softening it with base exchange Zeolite-like material. The soaked material and the dry glauconite may be conveyed by other means than a belt conveyor or elevator, for example it may be conveyed by gravity flow or hydraulically. In the latter case, of course, alkaline solution should be used. Once the speeds of iow of the solution and of feed of .the glauconite tions.

have been adjusted to the correct amount, the apparatus requires practically no supervision.y

Figure 2 shows'an apparatus diagrammatieally in which there are small modifica- The raw material is loaded into un'- derground tanks 26 through sicves 27 for the removal of gross impurity. Such a tank 26 may have conveniently a capacity of one days output of the separating apparatus to be employed. Assume that the tank 26 contains 12 tons of the screened glauconite; the latter' is allowed to standV for 12 hours or longer in the tank with sufficient' of the alkaline solution of the strength indicated above for easy soaking. For example, withthe l12 tons of screened mineral about 9 tons of water may be added containing about 6% pounds of caustic soda.` i

After the thorough soaking and standing the soaked minerali mass is raised from the tank26 by the belt conveyor 2 and 'discharged at constant speed into the cone 12 at the 'top of the separating column 11. The process then goes on which is described in connection With Figure 1 and as far as possible the same reference numerals have been employed.

' In this case the water entering'the conical vessel 16 by way of the pipe 17 is shown coming in at the top of the vessel 16and the coarser sand is shown discharged through the pipe 18 in the form of-a. swan neck at the bottom of the container 16.. The liquid containing the fine constituents isshown as passing through two receptacles 21 and 2S in series, the receptacle 28 receiving some of the line mud which is carried over from the receptacle 21.

If the coarser material separatd in the apparatus shown in Figures 1 and 2 be introduced into a colulmn of water or alkaline' solution-'moving upwards at a speed of 16 centimeters per second, only the heavy pan ticles will fall in the opposite direction to the movement ofthe solution and in general it will be found that such heavy particles are devoid of base exchange properties. Clearly therefore, if the soaked mineral mass be subjected in succession to the effect of columns of alkali solution or water moving re-l spectively at 1.75 centimeters per second as described with reference to Figures 1 and 2 and then at 16 centimeters per second, the commercially Iuseful fraction of the natural mineral can be separated from the clay and the Iinely divided constituents in the first column as described in connection with Figures 1 and 2 and from the heavy impurities in the second column. AIt .is also equally clear that by means of intermediate treatments at intermediatespeed's, the commercially useful fraction for base exchange can be separated into any desired number of grades with respect to their natural rates of lili',

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or funnel 32 for discharging the heavy in' active particles of the crude glauconite. Thusthle clay and extremely line particles are separated out by the rst or upper relatively long column in which the rate of flow is adjusted to a suitable value for this purpose.` Thesesclay-like and .tine impurities pass out at the top `of the column 11 into ythe tank quite so fine areseparated out at the top of the second columnlla and escape at the y swan neck 18a. The second short column 11b f separated `dlingswhich escape at 18, While,

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vpeptising vstep-can separates out the fine and light middlings which escape at 1-8? and the third short column 11c separates outi the heavy midas already indicated, the heavy inactive materials pass to the Achute 32 at the bottom.

It has already been ind'cated that the invention is not limited to"any of the forms of apparatus described and in the treatment materials other than base y exchange bodies, ofcourse, the peptising treatment has no part and, as already mentioned, even in the case of the washing and grading of base exchange bodies, suc-h as glauconite, the be omitted although l.thc thoroughness of separation is then to some extent sacrificed. It is only essential inaccordance with the invention that the apparatus be suitable for allowing the mass to be to b e submitted to the selective action of a column or of a number of columns quite short and The column 1l"v opens outatin succession of liquid movin with regulated speeds, so arranged that t lose portions of the mass, the natural rate of fall of which is less than the countenilow of the respective liquid columns, are conveyed by each column in the opposite direction to those portions having a greater rate of all than that of the movement of the liquidcolumn in the opposite direction and that those portions which are so moved in opposite directions shall be collected separately.

` Having thus described my invention, What I claim as new and desire to secure by Letters Patent 'is f 1. A process for separating out the clay constituents of crude glauconite from the mineral proper, consisting in treating the crude glauconite with a peptising agent and then subjecting it to the selective actionof a column of liquid rising at uniform speed 14. The particles which are not\ so that the particles or grains of the mineral proper whosematural rate of fall is-greater thanthe upward speed of the liquid column descendand are thereby freed from' the clay constituents Whose natural rate'of fall is less than vthe upward speed of theliquid column ivliich are consequently carried up by the latter.

ZAJ-proccss for separating out the clay constituents of crude glauconite from the mineral. proper, consisting in subjecting the crude glauconite to the selective action of an upwardly flowing column of weak alkaline solution rising at uniform speed so that the particles or grains of the mineral proper Whose natural rate of fall is greater than the upward speed of the liquid column descend and .are thereby freed from the clay constituents Whose `natural rate of fall is less than the upward speed of theliquidcolumn which are consequently carried up by the latter.

In witness whereof I hereunto subscribe'v my name this 12th day of June, 1925.

l f ERIC BERKELEY HIGGINS.- 

